CN203720111U - Micro crystal growing furnace for measuring microscopic structure of crystal growth boundary layer in situ in real time by using GIXRD (Grazing Incident X Ray Diffraction) technology - Google Patents
Micro crystal growing furnace for measuring microscopic structure of crystal growth boundary layer in situ in real time by using GIXRD (Grazing Incident X Ray Diffraction) technology Download PDFInfo
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- CN203720111U CN203720111U CN201320828702.XU CN201320828702U CN203720111U CN 203720111 U CN203720111 U CN 203720111U CN 201320828702 U CN201320828702 U CN 201320828702U CN 203720111 U CN203720111 U CN 203720111U
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- 239000013078 crystal Substances 0.000 title claims abstract description 53
- 238000002441 X-ray diffraction Methods 0.000 title abstract description 3
- 238000009304 pastoral farming Methods 0.000 title abstract description 3
- 239000013081 microcrystal Substances 0.000 title abstract 3
- 238000011065 in-situ storage Methods 0.000 title abstract 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000010410 layer Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000001341 grazing-angle X-ray diffraction Methods 0.000 claims description 15
- 238000002109 crystal growth method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- 239000011229 interlayer Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 239000010431 corundum Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 230000005496 eutectics Effects 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 3
- 239000000155 melt Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 11
- 239000010408 film Substances 0.000 description 6
- 230000005469 synchrotron radiation Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009605 growth rhythm Effects 0.000 description 1
- 238000012625 in-situ measurement Methods 0.000 description 1
- 238000000370 laser capture micro-dissection Methods 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model discloses a micro crystal growing furnace for measuring the microscopic structure of a melt crystal growth boundary layer in situ in real time by using a GIXRD (Grazing Incident X Ray Diffraction) technology, and belongs to the field of experimental equipment for detecting the microscopic structures of substances in real time. In the micro crystal growing furnace, a top heating way is adopted to uniformly melt the upper surface of an experimental crystal to form a layer of film, and a melt, a boundary layer and a crystal can be formed from the surface of the film to the crystal. Glancing incidence scanning is performed on the surface of the crystal as well as the film by adopting X rays in different incident angles, so that diffraction spectra at different depths of the film, the corresponding degree of order of different depths of the film as well as the change of the degree of order can be acquired respectively.
Description
Technical field
The utility model relates to the minicrystal growth furnace that a kind of GIXRD technology original position is measured crystal growth boundary layer micromechanism in real time, belongs to the experimental facilities field that material microstructure original position is measured in real time.
Background technology
When melt method for crystal growth, between crystal and melt, there is crystal growth boundary layer---the transition bed being transformed to crystal structure by melt structure.Structural motif in melt has progressively formed the growth unit with some crystal unit cell architectural feature after entering boundary layer, is finally superimposed on plane of crystal and forms crystal.Macroscopical growth rhythm of crystal is relevant to the Changing Pattern of the micromechanism of growth unit in boundary layer.Micromechanism and Changing Pattern thereof that original position is measured crystal growth boundary layer are in real time the experimental techniques of research crystal growth microscopic mechanism, are the experiment basis of setting up real crystal growth theory.
Within 1998, professor Yu Xiling of Shandong University designs a set of glass crystallizer, adopt holographic phase contrast interference microscopy, find that the growth of aqua-solution method crystal exists solute boundary layer, and applied for that patent of invention and practical patent, the patent No. are respectively 98110030.9,98220096.X.Calendar year 2001 peace light has been invented the method for growth unit microstructure change and Changing Pattern in application high-temperature laser micro Raman spectra real-time in-situ measurement crystal growing process, and adapt to crystal that high temperature Raman original position measures the in real time hot table apparatus of growing, the micromechanism in the melt of tens kinds of crystal, crystal and boundary layer has been carried out to real-time monitored and research, obtained important achievement in research.The method and device have obtained respectively patent of invention and practical license, and the patent No. is respectively ZL01238010.5, ZL01113657.X.
Raman spectrum is the reflection of chemical bond vibrational state between material particle, by Raman spectrum, can obtain the information of the structure of matter, therefore applying laser capture microdissection Raman spectroscopy can be in crystal growing process, and original position, real-time monitored are carried out in crystal, boundary layer, melt micromechanism and variation thereof.But the measured micromechanism of the method is indirectly, need the result of other method to supplement and perfect, the present invention is by GIXRD(synchrotron radiation glancing incidence X-ray diffraction spectrum) technology original position measures the X-ray diffraction spectrum of the different depth of the film forming after plane of crystal fusing in real time, thereby obtain melt, growth boundary layer and the trizonal micromechanism information of crystal below surface, and the development law of growth unit micromechanism, be a kind of new method of research crystal growth microscopic mechanism.Can the grow experimental result of additive method of Study on Microcosmic Mechanism of crystal mutually be confirmed and be supplemented, crystal growth Study on Microcosmic Mechanism is improved and deeply more.
Summary of the invention
Technical problem to be solved in the utility model is to provide a kind of GIXRD technology original position to measure in real time method and the minicrystal growth furnace of crystal growth boundary layer micromechanism.
Technical problem to be solved in the utility model realizes by the following technical solutions:
A kind of GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time, it comprises body of heater, described body of heater top is provided with bell, described body of heater is provided with water inlet and water delivering orifice outward, it is characterized in that: described body of heater one side has into perforation, and its opposite side has perforation hole;
In described body of heater, have thermal insulation medium and electric heater, described electric heater is positioned at body of heater top, and body of heater below corresponding thereto is also provided with for holding the crucible of crystal wafer;
Described electric heater is a rectangle corundum that is wound with electrical heating wire.
Described electrical heating wire two ends and extraneous temperature control system join.
Described body of heater is double-layer furnace body, and between double-layer furnace body, forms interlayer, and this interlayer communicates with water inlet and water delivering orifice on body of heater, and the water inlet on described body of heater and water delivering orifice and extraneous circulating water cooling system join.
Described crucible side also has thermopair, the monitoring of in real time temperature of sample vicinity being carried out by thermopair.
Described perforation hole bore is greater than into perforation.
Described thermal insulation medium is foamed alumina material or foam zirconia material, and crucible is the crucible not reacting with sample generation eutectic.
In order to adapt to the requirement for experiment condition at synchrotron radiation X-ray glancing incidence line station, the size of its body of heater is 70mm*30mm*50mm.
Plane of crystal temperature can regulate according to extraneous temperature control system, the highlyest at present can rise to 1400 ℃, temperature error ± 0.1 ℃ of temperature measuring point while guaranteeing constant temperature.
While making the work of minicrystal growth furnace by adjusting circulating water cooling system, temperature and the room temperature of outside surface are suitable.
The beneficial effects of the utility model are:
1) melt, boundary layer and the trizonal micromechanism of crystal when the utility model is realized the growth of original position real-time monitored crystal by synchrotron radiation glancing incidence X-ray diffraction spectral technology;
2) this minicrystal growth furnace adopts the design of accurate temperature and accurate temperature control instrument, test sample forms stable melt, boundary layer and crystal three subregions of mobile equilibrium, and fine setting grazing angle just can original position be measured this trizonal diffraction spectra in real time.
Accompanying drawing explanation
Fig. 1 is the utility model structural representation;
Fig. 2 is the utility model double-layer furnace body structural representation;
Fig. 3 is the utility model lateral parts structural representation;
Fig. 4 is structure for amplifying schematic diagram after crystal prototype heating.
In figure: 1-body of heater; 101-interlayer; 2-bell; 3-water inlet; 4-water delivering orifice; 5-enters perforation; 6-perforation hole; 7-thermal insulation medium; 8-electric heater; 801-electrical heating wire; 802-rectangle corundum; 9-crucible; 10-thermopair; 11-crystal prototype; The film of 12-fusing; 1201-melt; 1202-boundary layer.
Embodiment
For technological means, creation characteristic that the utility model is realized, reach object and effect is easy to understand, below in conjunction with concrete diagram, further set forth the utility model.
As Figure 1-4, a kind of GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time, it comprises body of heater 1, body of heater 1 top is provided with bell 2, outer water inlet 3 and the water delivering orifice 4 of being provided with of body of heater 1, body of heater 1 one sides have into perforation 5, and its opposite side has perforation hole 6;
In body of heater 1, have thermal insulation medium 7 and electric heater 8, electric heater 8 is positioned at body of heater 1 top, and body of heater 1 below corresponding thereto is also provided with for holding the crucible 9 of crystal wafer.
Electric heater 8 is rectangle corundum 802 that are wound with electrical heating wire 801, be placed in the top of crystal prototype, by electric current heat-dissipating, form the gradient temperature field of upper heat and lower cold, can in the molten film on plane of crystal and top thereof, form three stable subregions of crystal, boundary layer and melt.
Electrical heating wire 801 two ends and extraneous temperature control system join.According to heating-up temperature, also can change to some extent with the different electrical heating wire here of atmosphere configuration.
Body of heater 1 is double-layer furnace body, and between double-layer furnace body, forms interlayer 101, and this interlayer 101 communicates with water inlet 3 and water delivering orifice 4 on body of heater 1, and the water inlet 3 on body of heater 1 joins with water delivering orifice 4 and extraneous circulating water cooling system.
Crucible 9 sides also have thermopair 10, the monitoring of in real time temperature of crystal prototype 11 vicinity being carried out by thermopair 10.
The needs that gather in order to meet diffraction information, perforation hole 6 bores are greater than into perforation 5.
Thermal insulation medium 7 is foamed alumina material or foam zirconia material, and crucible 9 is the crucible not reacting with sample generation eutectic.
In order to adapt to the requirement for experiment condition at synchrotron radiation X-ray glancing incidence line station, the size of its body of heater 1 is 70mm*30mm*50mm.
Plane of crystal temperature can regulate according to extraneous temperature control system, the highlyest at present can rise to 1400 ℃, temperature error ± 0.1 ℃ of temperature measuring point while guaranteeing constant temperature.
While making the work of minicrystal growth furnace by adjusting circulating water cooling system, temperature and the room temperature of outside surface are suitable.
The utility model is put into the crystal prototype polishing on the crucible 9 of minicrystal growth furnace, makes crystal prototype 11 upper surfaces keep basic horizontal; Again minicrystal growth furnace is put on the platform at synchrotron radiation X-ray grazing-incidence diffraction line station, fine tuning micro furnace position, make X ray with special angle glancing incidence to crystal upper surface, then close X ray light source; Open the cooling water system electric heater 8 of unifying, by electric heater 8, make the fusing of crystal upper surface form thin film 12, the thickness of film 12 can be controlled by the power of electric heater 8, makes it to form from top to down three subregions of melt 1201, boundary layer 1202 and crystal; Open X ray light source, fine setting incident angle size glancing incidence, to different depth place and the crystal interface of film, collects the diffraction spectrum of melt 1201, boundary layer 1202 and the crystal of the film 12 following different depths in surface, and then obtains their micromechanism information.
More than show and described ultimate principle of the present utility model and principal character and advantage of the present utility model.The technician of the industry should understand; the utility model is not restricted to the described embodiments; that in above-described embodiment and instructions, describes just illustrates principle of the present utility model; do not departing under the prerequisite of the utility model spirit and scope; the utility model also has various changes and modifications, and these changes and improvements all fall within the scope of claimed the utility model.The claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (6)
1.GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time, it comprises body of heater, described body of heater top is provided with bell, described body of heater is provided with water inlet and water delivering orifice outward, it is characterized in that: described body of heater one side has into perforation, and its opposite side has perforation hole;
In described body of heater, have thermal insulation medium and electric heater, described electric heater is positioned at body of heater top, and body of heater below corresponding thereto is also provided with for holding the crucible of crystal wafer;
Described electric heater is a rectangle corundum that is wound with electrical heating wire.
2. GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time according to claim 1, it is characterized in that: described electrical heating wire two ends and extraneous temperature control system join.
3. GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time according to claim 1, it is characterized in that: described body of heater is double-layer furnace body, and between double-layer furnace body, form interlayer, this interlayer communicates with water inlet and water delivering orifice on body of heater, and the water inlet on described body of heater and water delivering orifice and extraneous circulating water cooling system join.
4. GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time according to claim 1, it is characterized in that: described crucible side also has thermopair, the monitoring of in real time temperature of sample vicinity being carried out by thermopair.
5. GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time according to claim 1, it is characterized in that: described perforation hole bore is greater than into perforation.
6. GIXRD technology original position is measured the minicrystal growth furnace of crystal growth method by melt boundary layer micromechanism in real time according to claim 1, it is characterized in that: described thermal insulation medium is foamed alumina material or foam zirconia material, crucible is the crucible not reacting with sample generation eutectic.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320828702.XU CN203720111U (en) | 2013-12-16 | 2013-12-16 | Micro crystal growing furnace for measuring microscopic structure of crystal growth boundary layer in situ in real time by using GIXRD (Grazing Incident X Ray Diffraction) technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320828702.XU CN203720111U (en) | 2013-12-16 | 2013-12-16 | Micro crystal growing furnace for measuring microscopic structure of crystal growth boundary layer in situ in real time by using GIXRD (Grazing Incident X Ray Diffraction) technology |
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| CN203720111U true CN203720111U (en) | 2014-07-16 |
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| CN201320828702.XU Expired - Lifetime CN203720111U (en) | 2013-12-16 | 2013-12-16 | Micro crystal growing furnace for measuring microscopic structure of crystal growth boundary layer in situ in real time by using GIXRD (Grazing Incident X Ray Diffraction) technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103698348A (en) * | 2013-12-16 | 2014-04-02 | 中国科学院合肥物质科学研究院 | Method for measuring microstructure of crystal growth boundary layer in situ and in real time by GIXRD (grazing incidence X-ray diffraction) technology and minitype crystal growing furnace |
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- 2013-12-16 CN CN201320828702.XU patent/CN203720111U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103698348A (en) * | 2013-12-16 | 2014-04-02 | 中国科学院合肥物质科学研究院 | Method for measuring microstructure of crystal growth boundary layer in situ and in real time by GIXRD (grazing incidence X-ray diffraction) technology and minitype crystal growing furnace |
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Granted publication date: 20140716 |
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